CN209522923U - Microwave plasma CVD device - Google Patents

Microwave plasma CVD device Download PDF

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Publication number
CN209522923U
CN209522923U CN201820640319.4U CN201820640319U CN209522923U CN 209522923 U CN209522923 U CN 209522923U CN 201820640319 U CN201820640319 U CN 201820640319U CN 209522923 U CN209522923 U CN 209522923U
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resonant cavity
plasma cvd
cvd device
microwave plasma
microwave
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马懿
马修·L·斯卡林
朱金华
吴建新
缪勇
卢荻
艾永干
克里斯托弗·E·格里芬
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Suzhou Beilaike Diamond Technology Co ltd
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Suzhou Berik Crystal Drilling Technology Co Ltd
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Abstract

This application discloses a kind of microwave plasma CVD devices, including resonant cavity, coupling conversion chamber and the medium window being separated between resonant cavity and coupling conversion chamber, the medium window has a cooling cavities, the cooling cavities is independently of the resonant cavity and coupling conversion chamber, the cooling cavities has the inlet and outlet that can be connected to external cooling circuit, the material of the medium window is quartz glass, and the external cooling circuit is the gas return path of refrigeration.The cooling to medium window may be implemented by the cooling gas flowed in the utility model, improves the heat-resisting ability of medium window.Due to solving the problems, such as the cooling of quartz glass, it can solve pumping low vacuum problem in waveguide, to conducting electromagnetic wave as perturbation of the flowing for electromagnetic wave in vacuum, solving previous cooling air fluid, there is great effect for the stabilization of plasma.

Description

Microwave plasma CVD device
Technical field
The application belongs to the synthesis technical field of single-crystal diamond, more particularly to a kind of microwave plasma chemical gas phase Precipitation equipment and its application.
Background technique
The microwave waveguide transmissions that microwave plasma CVD (MPCVD) generates microwave generator are to anti- Device is answered, and is passed through CH into reactor4With H2Mixed gas, high-intensitive microwave energy excitation decomposes the carbon containing gas above substrate The Viability carbon-containing group of the bodily form and atom state hydrogen, and plasma is formed, to obtain diamond thin in deposition on substrate.
In single-crystal diamond synthesis process, the medium window in resonant cavity is easy fever, and the prior art is usually in resonance Cooling air fluid is passed through in chamber to cool down medium window, and the flowing of cooling air fluid can generate electromagnetic wave Perturbation has significant effect the stabilization of plasma.
Utility model content
The purpose of this utility model is to provide a kind of microwave plasma CVD devices, to overcome existing skill Deficiency in art.
To achieve the above object, the utility model provides the following technical solutions:
The embodiment of the present application discloses a kind of microwave plasma CVD device, including resonant cavity, coupling conversion Chamber and the medium window being separated between resonant cavity and coupling conversion chamber,
The medium window has a cooling cavities, which converts chamber independently of the resonant cavity and coupling,
The cooling cavities has the inlet and outlet that can be connected to external cooling circuit.
Preferably, in above-mentioned microwave plasma CVD device, the material of the medium window is stone English glass.
Preferably, in above-mentioned microwave plasma CVD device, the medium window includes upper layer stone English glass and lower layer's quartz glass, upper layer quartz glass and lower layer's quartz glass surround the cooling cavities.
Preferably, in above-mentioned microwave plasma CVD device, the external cooling circuit is refrigeration Gas return path.
Preferably, in above-mentioned microwave plasma CVD device, process gas passes through vortex air inlet side Formula enters the resonant cavity, and process gas, which is excited to discharge in resonant cavity, forms spherical plasma.
Preferably, in above-mentioned microwave plasma CVD device, the coupling conversion chamber passes through water cooling Mode temperature control.
Preferably, in above-mentioned microwave plasma CVD device, the vacuum-pumping pipeline of the resonant cavity On be provided with a sealing plate, at least one stomata is offered on the sealing plate.
Preferably, in above-mentioned microwave plasma CVD device, one is offered on the sealing plate Stomata, the diameter of the stomata are 0.5~1mm.
Preferably, in above-mentioned microwave plasma CVD device, the medium window and resonant cavity it Between by 1 be aluminium ring sealing.
Compared with the prior art, the advantages of the utility model are: the utility model can be with by the cooling gas of flowing It realizes the cooling to medium window, improves the heat-resisting ability of medium window.It, can due to solving the problems, such as the cooling of quartz glass To solve the problems, such as to take out low vacuum in waveguide, thus by electromagnetic wave in conduction as in vacuum, solving previous cooling air stream The flowing of body has great effect for the stabilization of plasma for the perturbation of electromagnetic wave.
Detailed description of the invention
In order to illustrate the technical solutions in the embodiments of the present application or in the prior art more clearly, to embodiment or will show below There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this The some embodiments recorded in application, for those of ordinary skill in the art, without creative efforts, It is also possible to obtain other drawings based on these drawings.
Fig. 1 show the structural representation of microwave plasma CVD device in the utility model specific embodiment Figure;
Fig. 2 show the cross-sectional view of medium window in the utility model specific embodiment;
Fig. 3 show the cross-sectional view of sealing plate in the utility model specific embodiment.
Specific embodiment
The technical solution of the utility model is clearly and completely described below in conjunction with attached drawing, it is clear that described Embodiment is the utility model a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, originally Field those of ordinary skill every other embodiment obtained without making creative work belongs to practical Novel protected range.
It is in the description of the present invention, it should be noted that term " center ", "upper", "lower", "left", "right", " perpendicular Directly ", the orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings, and is only For ease of description the utility model and simplify description, rather than the device or element of indication or suggestion meaning must have it is specific Orientation, be constructed and operated in a specific orientation, therefore should not be understood as limiting the present invention.In addition, term " the One ", " second ", " third " are used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " is pacified Dress ", " connected ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or integrally Connection;It can be mechanical connection, be also possible to be electrically connected;Can be directly connected, can also indirectly connected through an intermediary, It can be the connection inside two elements.For the ordinary skill in the art, above-mentioned art can be understood with concrete condition The concrete meaning of language in the present invention.
As shown in connection with fig. 1, microwave plasma CVD device includes microwave source 10, plasmon coupling device 20 and resonance device 30.
Microwave source 10 can be the equipment such as the microwave generator of this field routine for generating microwave, generated micro- The power of wave can be able to be 915MHz-2.45GHz for 6~75kW, frequency.
In the present embodiment, microwave source 10 generate microwave power be 6~10kW, frequency 2.45GHz.
Resonance device 30 includes a resonant cavity 31 and deposition table 32.
The shell of resonant cavity 31 can be made of metal material or quartz material.Preferably, resonant cavity is by metal material (example Such as aluminium or copper) it is made, to be conducive to carry out water-cooled process to resonant cavity.
The shape of resonant cavity 31 can be various shapes, such as cylindrical.
Plasmon coupling device 20 uses antenna manifold type.
Specifically, plasmon coupling device 20 includes waveguide, Mode-transducing antenna 21, coupling conversion chamber 22 and medium Window 23.
Wherein, waveguide is connected between microwave source 10 and coupling conversion chamber 22;The bottom end of Mode-transducing antenna 21 extends To coupling conversion chamber 22;Coupling conversion chamber 22 is set to the top of resonant cavity 31, and medium window 23 is located at resonant cavity 31 and coupling It closes between conversion chamber 22.
The medium window 23 at 31 top of resonant cavity is the window formed by translucent material (such as quartz or sapphire), energy Enough make microwave transparent hence into resonant cavity 31, and it also ensures the sealing performance of resonant cavity 31.
In the operating condition, coupling converts the operating pressure of chamber 22 as high vacuum (0.13~1.3 × 10-5Pa), resonant cavity 31 operating pressure is ultrahigh vacuum (operating pressure 1.3 × 10-5Pa~1.3 × 10-10Pa)。
Further, waveguide includes first wave conduit 24 and second waveguide pipe 25.
First wave conduit 24 is rectangular waveguide;Coupling converts chamber 22 as circular waveguide, and second waveguide pipe 25 is connected to Between the first wave conduit 24 and the top of coupling conversion chamber 22, the second waveguide pipe 25 is vertical with first wave conduit 24 to be set It sets;Mode-transducing antenna 21 and second waveguide pipe 25 are coaxially disposed.
Convert chamber 22 can be metal sidewall for coupling, and when chamber 22 is converted in setting coupling, Mode-transducing antenna 21 can be by The microwave of TE10 mode in first wave conduit 24 is converted to TEM mode, and is sent to coupling conversion chamber through second waveguide pipe 25 After 22, the microwave of TEM mode is converted to TM01 mode again by Mode-transducing antenna 21, hence into resonant cavity 31.This setting side Formula can be avoided the microwave that the microwave of TE10 mode is converted directly into the not corresponding TM01 mode of electric field, to make to be formed by The energy of TM01 modes microwave maximizes, and further increases the service efficiency of microwave energy.Also, the microwave of TM01 mode can So that 32 upper area of deposition table is formed the electromagnetic field of maximum intensity, and be conducive to excite ellipsoid or spherical plasma 34, Pollution is generated to the diamond thin of deposition so as to avoid the side wall of resonant cavity 31.
In one embodiment, tuner 26 is provided between first wave conduit 24 and microwave source 10, the tuner 26 to Adjust the waveform of the microwave transmitted in first wave conduit 24.
In the technical solution, tuner make to adjust the waveform of the microwave transmitted in first wave conduit 24 its with Mode-transducing antenna 21 matches, to make the microwave energy of input maximize, such as it can be three spiral shells of this field routine Follow closely impedance tuner etc..Three screw impedance tuners can manual tuning or automatic tuning.
In one embodiment, transition waceguide 28 is provided between tuner 26 and first wave conduit 24.It is preferred that the standard of using Transition waceguide WR340to 284.
In one embodiment, one end of first wave conduit 24 is provided with cooling trough, and lower part has low pressure to vacuumize interface.
In one embodiment, Mode-transducing antenna 21 is metal Coupling antenna.
In one embodiment, the side wall of coupling conversion chamber 22 is provided with water cooling plant 27.
In the technical solution, the side wall of coupling conversion chamber can be arranged to double-deck sandwich, interlayer space passes through The liquid for being passed through refrigeration carries out temperature control.The liquid of refrigeration is run in a looping fashion, has water guide water route, prevents from having in interlayer " dead Water " generates.
In another embodiment, plasmon coupling device 20 uses surface wave manifold type, and principle is: passing through microwave Circulator and waveguide are crossed, vacuum chamber is entered by coupling aperture under the adjusting of waveguide short piston, when microwave power is sufficiently large When, compared under low pressure can gas breakdown electric discharge, and short-circuit plunger adjusting under form high-density plasma.
In another embodiment, plasmon coupling device 20 uses direct coupling type, and principle is: making microwave through wave Conduit enters in the vacuum of sealing through quartz window, and in the case where the short-circuit plunger of waveguide pipe end is adjusted, direct-coupling excitation is generated Plasma, however its adjusting tool that there is output power-adjustable range small, to formation plasma acquires a certain degree of difficulty, film The defects of degree of purity and limited depositional area.
As shown in connection with fig. 2, medium window 23 has a cooling cavities 231, and the surrounding of medium window 23 is formed with and cooling The gas feed 232 and gas vent 233 that cavity 231 is connected to.
Further, it is connected to outside the inlet and outlet of cooling cavities 231 and resonant cavity, the closed cavity constituted is independent In resonant cavity and coupling conversion chamber, therefore, cooling cavities to resonant cavity and will not couple conversion chamber when being passed through cooling gas Pressure, which is constituted, to be influenced.
In the technical solution, the cooling to medium window may be implemented by the cooling gas of flowing, improve medium window Heat-resisting ability.
Due to solving the problems, such as the cooling of quartz glass, pumping low vacuum problem in waveguide can solve, thus by electromagnetic wave In conduction as perturbation of the flowing for electromagnetic wave in vacuum, solving previous cooling air fluid, for it is equal from The stabilization of daughter has great effect.
Further, medium window preferably uses double-deck quartz glass, by 1 is aluminium ring between quartz glass and resonant cavity Sealing, so as to realize the sealing of ultrahigh vacuum.
It is necessary, high-purity process gas inlets are also communicated on resonant cavity 31, gas feed is that surrounding is vortexed into cavity, Each aperture is about 0.5~1mm of diameter, and circumferencial direction is uniformly distributed general 8~10.
It is necessary, it is additionally provided on resonant cavity 31 and vacuumizes interface, vacuumized interface and be connected to by pipeline with vacuum pump.
As shown in connection with fig. 3, in a preferred embodiment, proportioning valve is provided on vacuum line, proportioning valve offers for one The sealing plate 33 of stomata 331.
In the technical solution, by the sealing plate of aperture, the pressure of control cavity on the one hand can be very good, on the other hand Greatly reduce cost.
In a preferred embodiment, a stomata is offered on sealing plate, the diameter of the stomata is 0.5~1mm.
In other embodiments, the quantity of stomata and the size of stomata can require to adjust according to vacuum pressure.
The working principle and process of above-mentioned microwave plasma CVD equipment are as follows: resonant cavity 31 is carried out first It vacuumizes, and is passed through the mixed gas of methane and hydrogen composition into resonant cavity 31, microwave is then generated by microwave source 10, it is micro- Microwave caused by wave source 10 is propagated in first wave conduit with TE10 mode, after the conversion of Mode-transducing antenna 21, It is propagated in second waveguide pipe 25, after entering coupling conversion chamber 22, is converted again through Mode-transducing antenna 21 in a tem mode For TM01 mode, enter resonant cavity 31, the activity of methane formation carbon-containing group and atom of 32 top of deposition table through medium window 23 State hydrogen, and spherical plasma 34 is formed, to deposit to obtain diamond thin in seed crystal upper surface.
Specifically, the present embodiment also provides single-crystal diamond synthetic method, comprising steps of
(1), the planarizing process such as mechanical lapping seed crystal (substrate) surface polishing: are carried out to diamond seed surface;
(2), 100 acid processing: are heated to water-sulfuric acid-hydrogen peroxide mixed solution (ratio are as follows: 1:5:1) temperature of heating It~130 degree, cleans 10~20 minutes;
(3), seed crystal deionized water is rinsed 10~15 minutes;
(4), it is ultrasonically treated: (such as: isopropanol) carrying out ultrasonic cleaning 30 minutes in organic solvent.
(5), deionized water is rinsed 6~10 minutes;
(6), dustless oven temperature is heated to 80 degree of bakings 10~30 minutes;
(7), resonant cavity is opened, seed crystal is fixed on to the upper surface of deposition table;
(8), cavity is closed;
(9), low-voltage vacuum is taken out in first wave conduit;
(10), water-cooling shaft is adjusted to suitable position, to control the temperature of seed crystal;
(11), resonant cavity is cleaned with high-purity hydrogen, can be cleaned multiple times by several times or once cleaned.As primary cleaning is taken out Vacuum is to 0.0015Torr;Hydrogenation to 5Torr, then in control chamber body stable gas pressure in 5Torr;
(12), microwave source is opened, three needle tuners are adjusted, excites resonant cavity plasma ignition.General plasma ignition hair Life is in 5~10torr.
(13), increase power according to the following table 1, adjust air pressure, coupled and adjusted by power air pressure, it is ensured that plasma is not It can loss.
Table 1
Plasma power 600w 1000w 1500w 2000w 2500w 3000w 3500w~8000w
Air pressure 10torr 20torr 50torr 100torr 120torr 150torr 150torr
(14), the position for finely tuning microwave power and water-cooling shaft controls seed temperature by double-colored sensor.
(15), with hydrogen etched seed surface 15min.
(16), 800~1400 degree of seed temperature are controlled.
(17), process gas 50scmm methane, 500sccm hydrogen, diamond continued propagation are passed through.
(18), resonant cavity is opened after completing growth.
Finally, it should be noted that the above various embodiments is only to illustrate the technical solution of the utility model, rather than it is limited System;Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should Understand: it is still possible to modify the technical solutions described in the foregoing embodiments, or to some or all of Technical characteristic is equivalently replaced;And these are modified or replaceed, it does not separate the essence of the corresponding technical solution, and this is practical new The range of each embodiment technical solution of type.

Claims (10)

1. a kind of microwave plasma CVD device, which is characterized in that including resonant cavity, coupling conversion chamber and The medium window being separated between resonant cavity and coupling conversion chamber,
The medium window has a cooling cavities, which converts chamber independently of the resonant cavity and coupling,
The cooling cavities has the inlet and outlet that can be connected to external cooling circuit,
The material of the medium window is quartz glass,
The external cooling circuit is the gas return path of refrigeration.
2. microwave plasma CVD device according to claim 1, which is characterized in that the medium window Including upper layer quartz glass and lower layer's quartz glass, upper layer quartz glass and lower layer's quartz glass surround the cooling cavities.
3. microwave plasma CVD device according to claim 1, which is characterized in that process gas passes through Vortex intake method enters the resonant cavity, and process gas, which is excited to discharge in resonant cavity, forms spherical plasma.
4. microwave plasma CVD device according to claim 1, which is characterized in that the coupling conversion Chamber passes through water-cooling pattern temperature control.
5. microwave plasma CVD device according to claim 1, which is characterized in that the resonant cavity Vacuum-pumping tube road is provided with a sealing plate, at least one stomata is offered on the sealing plate.
6. microwave plasma CVD device according to claim 5, which is characterized in that on the sealing plate A stomata is offered, the diameter of the stomata is 0.5~1mm.
7. microwave plasma CVD device according to claim 5, which is characterized in that the medium window Passing through 1 between resonant cavity is aluminium ring sealing.
8. microwave plasma CVD device according to claim 1, which is characterized in that further include microwave Source, the power of microwave caused by microwave source are 6~75kW, and frequency is 915MHz~2.45GHz.
9. microwave plasma CVD device according to claim 8, which is characterized in that further include waveguide And Mode-transducing antenna, waveguide are connected between microwave source and coupling conversion chamber;The bottom end of Mode-transducing antenna extends to coupling It is intracavitary to close conversion.
10. microwave plasma CVD device according to claim 9, which is characterized in that the waveguide Including first wave conduit and second waveguide pipe, second waveguide pipe be connected to the first wave conduit and coupling conversion chamber top it Between, the second waveguide pipe is vertically arranged with first wave conduit, and Mode-transducing antenna and second waveguide pipe are coaxially disposed.
CN201820640319.4U 2018-05-02 2018-05-02 Microwave plasma CVD device Active CN209522923U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201820640319.4U CN209522923U (en) 2018-05-02 2018-05-02 Microwave plasma CVD device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201820640319.4U CN209522923U (en) 2018-05-02 2018-05-02 Microwave plasma CVD device

Publications (1)

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Effective date of registration: 20230918

Address after: Room 13, 3rd Floor, No. 232 Yuanfeng Road, Yushan Town, Kunshan City, Suzhou City, Jiangsu Province, 215347

Patentee after: Suzhou Beilaike Diamond Technology Co.,Ltd.

Address before: Room 711, Building D, No. 398 Ruoshui Road, Suzhou Industrial Park, Suzhou City, Jiangsu Province, 215000

Patentee before: SUZHOU BEILAIKE JINGZUAN TECHNOLOGY Co.,Ltd.

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